阅读说明：本技术 一种高温诱导钛锆基合金表面耐磨扩散层的制备方法 (Preparation method of high-temperature induced wear-resistant diffusion layer on surface of titanium-zirconium-based alloy ) 是由 钟华 马明臻 张春鹏 刘日平 黄飞 胡恩柱 于 2020-06-24 设计创作，主要内容包括：本发明属于合金材料表面保护层的制备技术领域,具体的说是一种高温诱导钛锆基合金表面耐磨扩散层的制备方法；该制备方法采用的氧化炉包括壳体、电机、一号转轴、支撑板和注氧单元；所述一号转轴转动连接在壳体底端内侧壁上,且一号转轴与电机输出端固连；所述支撑板安装在一号转轴顶端侧壁上；所述注氧单元安装在壳体内侧壁上,注氧单元包括一号凸轮、气囊、储气室和固定板；在一号转轴的转动过程中带动支撑板同时进行转动,从而不断的更换方形试样和氧气之间的接触面积,实现氧气在方形试样表面的均匀分布,保证了方形试样表面真空扩散层的厚度均匀性,从而有效增加了方形试样表面的耐磨损度。(The invention belongs to the technical field of preparation of surface protection layers of alloy materials, and particularly relates to a preparation method of a high-temperature induced wear-resistant diffusion layer on the surface of a titanium-zirconium-based alloy; the oxidation furnace adopted by the preparation method comprises a shell, a motor, a first rotating shaft, a supporting plate and an oxygen injection unit; the first rotating shaft is rotatably connected to the inner side wall of the bottom end of the shell and is fixedly connected with the output end of the motor; the supporting plate is arranged on the side wall of the top end of the first rotating shaft; the oxygen injection unit is arranged on the inner side wall of the shell and comprises a first cam, an air bag, an air storage chamber and a fixing plate; the rotation in-process at a pivot drives the backup pad and rotates simultaneously to continuous change area of contact between square sample and the oxygen, realize the evenly distributed of oxygen on square sample surface, guaranteed the thickness homogeneity of square sample surface vacuum diffusion layer, thereby effectively increased the stand wear and tear degree on square sample surface.)

1. A preparation method of a high-temperature induced wear-resistant diffusion layer on the surface of a titanium-zirconium-based alloy is characterized by comprising the following steps: the preparation method comprises the following steps:

s1: pressing high-purity metals of titanium, zirconium and aluminum with the purity of 99.5 percent and 50Al50V of intermediate alloy into short rod-shaped lump materials to obtain basic raw materials, manufacturing the basic raw materials into electrodes, and then carrying out smelting treatment through a vacuum consumable electrode arc furnace to obtain alloy ingots, wherein the smelting current is 180-260A, and the smelting time is 4-6 min;

s2: carrying out three-pier three-pull turning on the alloy ingot in the S1 to obtain a titanium-zirconium-based alloy bar, cutting a square sample with the shape of 10mm multiplied by 30mm from the bar by using a wire electric discharge machine, and then polishing the titanium-zirconium-based alloy square sample by using SiC abrasive paper to ensure that the surface roughness of the titanium-zirconium-based alloy square sample is 0.1-0.2 mu m;

s3: cleaning the titanium-zirconium-based alloy square sample in the step S2 in an ultrasonic cleaning machine to remove impurity particles on the surface of the titanium-zirconium-based alloy square sample, and drying the surface of the titanium-zirconium-based alloy square sample by using a hot air blower; wherein the heating temperature of the air heater is controlled to be 75-80 ℃, and an included angle of 45 degrees is formed between an air outlet of the air heater and the surface of the titanium-zirconium-based alloy square sample;

s4: carrying out thermal oxidation treatment on the titanium-zirconium-based alloy square sample in the S3 through a muffle furnace, wherein the heating temperature is 650-800 ℃, and the heat preservation time is 12 h; and after the heat preservation is finished, cooling the titanium-zirconium-based alloy square sample along with the furnace, after the titanium-zirconium-based alloy square sample is cooled to room temperature, putting the titanium-zirconium-based alloy square sample into an oxidation furnace for vacuum diffusion treatment, forming an oxygen diffusion layer on the surface of the titanium-zirconium-based alloy square sample, and finishing the preparation of the high-temperature induced titanium-zirconium-based alloy surface wear-resistant diffusion layer.

2. The method for preparing the high-temperature-induced wear-resistant diffusion layer on the surface of the titanium-zirconium-based alloy according to claim 1, wherein the method comprises the following steps: when the basic raw materials are smelted through a vacuum consumable electrode arc furnace, the smelting current is increased in stages, namely the smelting current is firstly 190A, and smelting is continued for 2 min; then the smelting current is increased to 230A, and smelting is continued for 2 min; and finally, increasing the smelting current to 260A, and finishing the smelting treatment of the basic raw materials after continuously smelting for 2 min.

3. The method for preparing the high-temperature-induced wear-resistant diffusion layer on the surface of the titanium-zirconium-based alloy according to claim 1, wherein the method comprises the following steps: in the vacuum diffusion process of the titanium-zirconium-based alloy square sample, the vacuum diffusion time is 8-10h, and the heating temperature is 400-550 ℃.

4. The method for preparing the high-temperature-induced wear-resistant diffusion layer on the surface of the titanium-zirconium-based alloy according to claim 1, wherein the method comprises the following steps: when the titanium-zirconium-based alloy square sample is cleaned by an ultrasonic cleaning machine, the titanium-zirconium-based alloy square sample needs to be cleaned by different cleaning liquids for three times; the method comprises the following steps of firstly cleaning the titanium-zirconium-based alloy square sample by using an acetone solution, cleaning the titanium-zirconium-based alloy square sample by using an alcohol solution after the cleaning is finished, and finally cleaning the titanium-zirconium-based alloy square sample by using deionized water.

5. The method for preparing the high-temperature-induced wear-resistant diffusion layer on the surface of the titanium-zirconium-based alloy according to claim 1, wherein the method comprises the following steps: the oxidation furnace comprises a shell (1), a motor (2), a first rotating shaft (3), a supporting plate (4) and an oxygen injection unit (5); an end cover (11) is arranged at the top end of the shell (1), and a support (12) is arranged at the bottom end of the shell (1); the motor (2) is arranged on the outer side wall of the bottom end of the shell (1); the first rotating shaft (3) is rotatably connected to the inner side wall of the bottom end of the shell (1), and the first rotating shaft (3) is fixedly connected with the output end of the motor (2); the supporting plate (4) is arranged on the side wall of the top end of the first rotating shaft (3); the oxygen injection unit (5) is arranged on the inner side wall of the shell (1), and the oxygen injection unit (5) comprises a first cam (51), an air bag (52), an air storage chamber (53) and a fixing plate (54); the first cam (51) is fixedly connected to the first rotating shaft (3); the air bag (52) is arranged on the inner side wall of the shell (1) close to the first cam (51), and oxygen is filled in the air bag (52); the air storage chamber (53) is arranged on the outer side wall of the shell (1), and the air storage chamber (53) is communicated with the air bag (52) through a hose; the fixing plate (54) is arranged on the inner side wall of the shell (1) close to the air storage chamber (53), a plurality of air nozzles (55) are arranged on the side wall of the fixing plate (54), and the air nozzles (55) are communicated with the air storage chamber (53).

6. The method for preparing the high-temperature-induced wear-resistant diffusion layer on the surface of the titanium-zirconium-based alloy according to claim 5, wherein the method comprises the following steps: a first sliding groove (541) is formed in the fixing plate (54); a clamping plate (542) is connected in the first sliding groove (541) in a sliding manner through a spring, and a second rotating shaft (543) is rotatably connected on the side wall of the first sliding groove (541) close to the air storage chamber (53); a plurality of openings (544) are arranged on the clamping plate (542) so that the air jet (55) penetrates through the openings (544); no. two cams (545) are installed to the tip that No. two pivot (543) are located first spout (541), and flabellum (546) are installed to the tip that No. two pivot (543) are located air receiver (53).

7. The method for preparing the high-temperature-induced wear-resistant diffusion layer on the surface of the titanium-zirconium-based alloy according to claim 5, wherein the method comprises the following steps: a positioning plate (41) is arranged on the supporting plate (4); a second sliding groove (411) is formed in the surface of the positioning plate (41), and the second sliding groove (411) is communicated with the air bag (52) through a hose; a plurality of first sliding blocks (412) and second sliding blocks (413) are connected in the second sliding groove (411) in a sliding mode; the first sliding block (412) is symmetrically and slidably connected to two ends of the second sliding groove (411), and elastic sealing cloth (414) is connected between the first sliding block (412) and the inner side wall of the second sliding groove (411); the second sliding block (413) is connected in a second sliding groove (411) between the first sliding blocks (412) in a sliding mode, and elastic sealing cloth (414) is connected between the second sliding block (413) and the first sliding blocks (412); the first sliding block (412) and the second sliding block (413) are internally provided with air holes (415), and the first sliding block (412) is connected with the second sliding block (413) through a V-shaped elastic plate (416).

8. The method for preparing the high-temperature-induced wear-resistant diffusion layer on the surface of the titanium-zirconium-based alloy according to claim 7, wherein the method comprises the following steps: a through hole (417) is formed in the side wall of the top end of the second sliding block (413), so that the through hole (417) is communicated with the air hole (415); a rubber plug (418) is connected in the through hole (417) in a sliding way; the V-shaped elastic plate (416) is connected to the side wall of the top end of the rubber plug (418).

Technical Field

The invention belongs to the technical field of preparation of surface protection layers of alloy materials, and particularly relates to a preparation method of a high-temperature induced wear-resistant diffusion layer on the surface of a titanium-zirconium-based alloy.

Background

The titanium alloy has the excellent characteristics of low density, high strength, good corrosion resistance and the like, and is an important structural material of an aerospace aircraft. The tensile strength of the Ti6Al4V titanium alloy which is widely used at present is 900-1100 MPa, and the failure elongation is 8-12%. The TiZrAlV alloy is a novel alloy material developed on the basis of Ti6Al4V alloy, and the introduction of zirconium element effectively improves the strength and hardness of the material, so that the TiZrAlV alloy becomes a candidate material of a very potential aerospace craft.

Disclosure of Invention

The invention provides a preparation method of a high-temperature induced wear-resistant diffusion layer on the surface of a titanium-zirconium-based alloy, aiming at improving the wear resistance of the titanium-zirconium-based alloy and prolonging the service life of the titanium-zirconium-based alloy in a use occasion with larger wear degree.

The technical scheme adopted by the invention for solving the technical problems is as follows: the invention relates to a preparation method of a high-temperature induced wear-resistant diffusion layer on the surface of a titanium-zirconium-based alloy, which comprises the following steps:

s1: pressing high-purity metals of titanium, zirconium and aluminum with the purity of 99.5 percent and 50Al50V of intermediate alloy into short rod-shaped lump materials to obtain basic raw materials, manufacturing the basic raw materials into electrodes, and then carrying out smelting treatment through a vacuum consumable electrode arc furnace to obtain alloy ingots, wherein the smelting current is 180-260A, and the smelting time is 4-6 min;

s2: carrying out three-pier three-pull turning on the alloy ingot in the S1 to obtain a titanium-zirconium-based alloy bar, cutting a square sample with the shape of 10mm multiplied by 30mm from the bar by using a wire electric discharge machine, and then polishing the titanium-zirconium-based alloy square sample by using SiC abrasive paper to ensure that the surface roughness of the titanium-zirconium-based alloy square sample is 0.1-0.2 mu m;

s3: cleaning the titanium-zirconium-based alloy square sample in the step S2 in an ultrasonic cleaning machine to remove impurity particles on the surface of the titanium-zirconium-based alloy square sample, and drying the surface of the titanium-zirconium-based alloy square sample by using a hot air blower; wherein the heating temperature of the air heater is controlled to be 75-80 ℃, and an included angle of 45 degrees is formed between an air outlet of the air heater and the surface of the titanium-zirconium-based alloy square sample;

s4: carrying out thermal oxidation treatment on the titanium-zirconium-based alloy square sample in the S3 through a muffle furnace, wherein the heating temperature is 650-800 ℃, and the heat preservation time is 12 h; and after the heat preservation is finished, cooling the titanium-zirconium-based alloy square sample along with the furnace, after the titanium-zirconium-based alloy square sample is cooled to room temperature, putting the titanium-zirconium-based alloy square sample into an oxidation furnace for vacuum diffusion treatment, forming an oxygen diffusion layer on the surface of the titanium-zirconium-based alloy square sample, and finishing the preparation of the high-temperature induced titanium-zirconium-based alloy surface wear-resistant diffusion layer.

Preferably, when the base raw material is smelted in a vacuum consumable electrode arc furnace, the smelting current is increased in stages, namely the smelting current is firstly 190A, and smelting is continued for 2 min; then the smelting current is increased to 230A, and smelting is continued for 2 min; and finally, increasing the smelting current to 260A, and finishing the smelting treatment of the basic raw materials after continuously smelting for 2 min.

Preferably, in the vacuum diffusion process of the titanium-zirconium-based alloy square sample, the vacuum diffusion time is 8-10h, and the heating temperature is 400-550 ℃.

Preferably, when the titanium-zirconium-based alloy square sample is cleaned by an ultrasonic cleaning machine, the titanium-zirconium-based alloy square sample needs to be cleaned by three different cleaning solutions; the method comprises the following steps of firstly cleaning the titanium-zirconium-based alloy square sample by using an acetone solution, cleaning the titanium-zirconium-based alloy square sample by using an alcohol solution after the cleaning is finished, and finally cleaning the titanium-zirconium-based alloy square sample by using deionized water.

Preferably, the oxidation furnace comprises a shell, a motor, a first rotating shaft, a supporting plate and an oxygen injection unit; the top end of the shell is provided with an end cover, and the bottom end of the shell is provided with a bracket; the motor is arranged on the outer side wall of the bottom end of the shell; the first rotating shaft is rotatably connected to the inner side wall of the bottom end of the shell and is fixedly connected with the output end of the motor; the supporting plate is arranged on the side wall of the top end of the first rotating shaft; the oxygen injection unit is arranged on the inner side wall of the shell and comprises a first cam, an air bag, an air storage chamber and a fixing plate; the first cam is fixedly connected to the first rotating shaft; the air bag is arranged on the inner side wall of the shell close to the first cam, and oxygen is filled in the air bag; the air storage chamber is arranged on the outer side wall of the shell, and the air storage chamber is communicated with the air bag through a hose; the fixed plate is arranged on the inner side wall of the shell close to the air storage chamber, and a plurality of air nozzles are arranged on the side wall of the fixed plate and communicated with the air storage chamber; the during operation, when needing to carry out the vacuum diffusion processing with the square sample of titanium zirconium base alloy, place square sample in the backup pad earlier, to the motor circular telegram again this moment, it rotates to drive a pivot after the motor circular telegram, a pivot drives a cam and carries out reciprocal extrusion to the gasbag in the rotation in-process, its inside oxygen passes through the jet orifice blowout after the gasbag pressurized, oxygen is through spouting back and square sample surface contact, thereby form one deck oxygen diffusion layer on its surface, and simultaneously, drive the backup pad and rotate simultaneously at the rotation in-process of a pivot, thereby continuous change the area of contact between square sample and the oxygen, realize the evenly distributed of oxygen on square sample surface, the thickness homogeneity on square sample surface vacuum diffusion layer has been guaranteed, thereby effectively increased the abrasion resistance on square sample surface.

Preferably, a first sliding groove is formed in the fixing plate; the first sliding groove is connected with a clamping plate in a sliding mode through a spring, and a second rotating shaft is rotatably connected to the side wall, close to the air storage chamber, of the first sliding groove; the clamping plate is provided with a plurality of openings, so that the air jet passes through the openings; a second cam is arranged at the end part of the second rotating shaft positioned in the first sliding groove, and fan blades are arranged at the end part of the second rotating shaft positioned in the air storage chamber; when the pneumatic air injection device works, after the motor is powered on, the first rotating shaft drives the first cam to rotate, the first cam realizes reciprocating extrusion on the air bag when rotating, the oxygen inside the air bag is pressed and enters the air storage chamber through the hose, the fan blade is driven to rotate in the oxygen flowing process, the fan blade drives the second cam to rotate through the second rotating shaft after rotating, the second cam realizes reciprocating extrusion on the clamping plate through matching with the spring in the rotating process, the reciprocating movement in the first sliding groove is realized after the clamping plate is extruded, the clamping plate produces stirring effect on the air injection port through the opening in the moving process, so that the air injection port can swing in a reciprocating mode in the shell, the flow rate and the flow range of the oxygen in the oxidation furnace are further increased, the oxidation effect on a square sample is enhanced, and the oxidation rate on the square sample is improved.

Preferably, the supporting plate is provided with a positioning plate; the surface of the positioning plate is provided with a second sliding groove which is communicated with the air bag through a hose; a plurality of first sliding blocks and second sliding blocks are connected in the second sliding groove in a sliding mode; the first sliding block is symmetrically and slidably connected to two ends of the second sliding groove, and elastic sealing cloth is connected between the first sliding block and the inner side wall of the second sliding groove; the second sliding block is connected in a second sliding groove between the first sliding blocks in a sliding manner, and elastic sealing cloth is connected between the second sliding block and the first sliding block; air holes are formed in the first sliding block and the second sliding block, and the first sliding block and the second sliding block are connected through a V-shaped elastic plate; when the device works, when a titanium-zirconium-based alloy square sample needs to be subjected to vacuum diffusion treatment, the square sample is placed on the V-shaped elastic plate, after the air bag is pressed, gas in the air bag enters the second sliding groove to generate thrust to the first sliding block, the first sliding block is stressed to slide in the second sliding groove in a reciprocating manner, in the sliding process of the first sliding block, the second sliding block is simultaneously thrust to the second sliding block through the V-shaped elastic plate, so that the second sliding block also slides in the second sliding groove, the V-shaped elastic plate is also correspondingly bent and elastically deformed, when the V-shaped elastic plate is bent and elastically deformed, the square sample generates jacking force and thrust, so that the square sample rolls back and forth on the surface of the V-shaped elastic plate, the side face of the square sample, which is in contact with the V-shaped elastic plate, is continuously replaced, and the side face of the square sample, which is in contact with the V-shaped elastic plate, cannot be fully contacted with, affecting the quality of the vacuum diffusion layer on the surface of the square sample.

Preferably, a through hole is formed in the side wall of the top end of the second sliding block, so that the through hole is communicated with the air vent; a rubber plug is connected in the through hole in a sliding manner; the V-shaped elastic plate is connected to the side wall of the top end of the rubber plug; the during operation, after oxygen gets into No. two spouts, make a slider and No. two sliders take place to slide under the effect of atmospheric pressure, thereby make V-arrangement elastic plate also take place corresponding elastic deformation, at the deformation in-process of V-arrangement elastic plate, V-arrangement elastic plate drives the rubber stopper and carries out reciprocal slip in the through-hole, thereby make and realize discontinuous intercommunication and jam between through-hole and the bleeder vent, when through-hole and bleeder vent intercommunication, oxygen in No. two spouts the bottom surface to square sample through-hole and bleeder vent, further strengthen the oxidation effect to square sample, guarantee the quality on square sample surface vacuum diffusion layer.

The invention has the following beneficial effects:

1. according to the preparation method of the high-temperature induced wear-resistant diffusion layer on the surface of the titanium-zirconium-based alloy, the oxidation treatment of the surface of the square titanium-zirconium-based alloy sample is realized through the cooperation of the shell, the motor, the first rotating shaft, the supporting plate and the oxygen injection unit, the quality of the vacuum diffusion layer on the surface of the square sample is enhanced, and the oxidation rate of the square sample is accelerated by improving the oxygen concentration on the surface of the square sample.

2. According to the preparation method of the high-temperature induced titanium-zirconium-based alloy surface wear-resistant diffusion layer, the air jet port can swing back and forth in the shell through the cooperation of the fixing plate, the clamping plate, the second rotating shaft, the fan blades and the second cam, the flow rate and the flow range of oxygen in the oxidation furnace are further increased, the oxidation effect on a square sample is enhanced, and the oxidation rate on the square sample is increased.

Drawings

The invention will be further explained with reference to the drawings.

FIG. 1 is a process flow diagram of the present invention;

FIG. 2 is a perspective view of an oxidation oven used in the present invention;

FIG. 3 is a sectional view of an oxidation oven used in the present invention;

FIG. 4 is an enlarged view of a portion of FIG. 3 at A;

FIG. 5 is a partial enlarged view at B in FIG. 3;

FIG. 6 is a surface topography of example 1 of the present invention;

FIG. 7 is a surface topography of example 2 of the present invention;

FIG. 8 is a surface topography of example 3 of the present invention;

in the figure: the oxygen injection device comprises a shell 1, an end cover 11, a support 12, a motor 2, a first rotating shaft 3, a support plate 4, a positioning plate 41, a second sliding groove 411, a first sliding block 412, a second sliding block 413, elastic sealing cloth 414, an air hole 415, a V-shaped elastic plate 416, a through hole 417, a rubber plug 418, an oxygen injection unit 5, a first cam 51, an air bag 52, an air storage chamber 53, a fixing plate 54, a first sliding groove 541, a clamping plate 542, a second rotating shaft 543, an opening 544, a second cam 545, fan blades 546 and an air jet 55.

Detailed Description

In order to make the technical means, the creation characteristics, the achievement purposes and the effects of the invention easy to understand, the invention is further described with the specific embodiments.